Method for preparing TiO2/g-C3N4 composite visible light catalyst

A g-c3n4, visible light technology, used in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of hidden safety hazards and high operational requirements for operators, and achieve light absorption rate and photocatalytic activity. High, simple process, many photocatalytic active centers

Active Publication Date: 2015-01-28

JIANGSU UNIVERSITY OF TECHNOLOGY

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The ammonium fluoride used in the preparation process of the preparation method is a highly tox...

Method used

See Fig. 3, the ultraviolet-visible diffuse reflectance spectrum of product shows, the TiO of present embodiment synthesis/g-C The visible light absorption area of composite visible light catalyst is from 390 to 550 nm, and the scope of visible ...

Abstract

The invention discloses a method for preparing a TiO2/g-C3N4 composite visible light catalyst. The method comprises the following steps: firstly, uniformly dispersing a titanium source and a nitrogen source in ethanol, and subsequently dropping water into ethanol so as to obtain a mixed material; evaporating to dry the mixed material in a stirring state so as to obtain a precursor; transferring the prepared precursor to a muffle furnace, and calcining for 0.5-12 hours at 300-800 DEG C in the muffle furnace, thereby obtaining the TiO2/g-C3N4 composite visible light catalyst. The TiO2/g-C3N4 composite visible light catalyst can be prepared while TiO2 and g-C3N4 are prepared, and the synthesis of the two compounds TiO2 and g-C3N4 and the preparation of the composite visible light catalyst are achieved at one step; the process is simple, and industrialization production is easy to achieve. The composite visible light catalyst disclosed by the invention is rich in photocatalytic activity center, relatively high in both light absorption rate and photocatalytic activity, and relatively high in photocatalytic degradation rate of organisms.

Application Domain

Physical/chemical process catalystsWater/sewage treatment by irradiation +1

Technology Topic

Photocatalytic degradationMuffle furnace +8

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Examples

Experimental program(7)
Comparison scheme(2)

Example

[0033] (Example 1)

[0034] Preparation of TiO in this example 2 /g-C 3 N 4 The method of composite visible light catalyst includes the following steps:

[0035] ① Preparation of precursors. Put 20mL Ti(OBu) 4 Disperse 20g melamine and 500mL in ethanol at 20℃ evenly, and then add Ti(OBu) under stirring. 4 Add 50 mL of water dropwise to ethanol and melamine to obtain a mixture; the mixture is evaporated to dryness in a water bath at 70°C to 85°C (80°C in this example) under stirring to obtain a precursor 。

[0036] ②Transfer the precursor prepared in step ① to the muffle furnace, and calcinate in the muffle furnace at 520℃ for 2h to obtain TiO 2 /g-C 3 N 4 Composite visible light catalyst.

[0037] The product prepared in this example was characterized: the transmission electron microscope (TEM) used for the characterization was a JEOL 2010 transmission electron microscope of JEOL Ltd.; the X-ray diffractometer was a D/MAX-2500PC type X-ray of Rigaku Company, Japan Diffractometer; the ultraviolet-visible spectrometer is a UV-2700 spectrometer of Shimadzu Corporation. The instruments used in the following examples and comparative examples are the same as above.

[0038] see figure 1 , In the XRD diffraction pattern of the product, 27.29° belongs to g-C 3 N 4 The (002) plane; at 25.34°, 37.76°, 48.14°, 55.12° and 62.76°, corresponding to anatase TiO 2 (101), (004), (200), (211) and (204) crystal planes; 36.12°, 41.22°, 56.66° belong to rutile TiO 2 (101), (111) and (220) crystal planes; therefore the product is g-C 3 N 4 , Anatase TiO 2 And rutile TiO 2 The mixture of crystals indicates that TiO was successfully prepared in this example 2 /g-C 3 N 4 Composite visible light catalyst.

[0039] see figure 2 , figure 2 It is the TEM spectrum of the product obtained after calcination in step ②, the black dots in the figure are nano-TiO 2 Particles, by figure 1 It can be clearly seen that the nano TiO in the product of this example 2 Particles are evenly distributed in graphite flake g-C 3 N 4 in.

[0040] see image 3 , The ultraviolet-visible diffuse reflectance spectrum of the product shows that the TiO synthesized in this example 2 /g-C 3 N 4 The visible light absorption region of the composite visible light catalyst ranges from 390 to 550 nm, and has a wide visible light absorption range and high intensity. The composite photocatalyst prepared in this embodiment can absorb a large amount of visible light when used, and is suitable for visible light photocatalytic degradation of organic pollutants.

[0041] In order to test the TiO prepared in this example 2 /g-C 3 N 4 Test the photocatalytic degradation of methylene blue: the photocatalytic reaction was carried out in a cylindrical glass reactor, with a 300 W xenon lamp as the light source, and the light source was 20cm away from the liquid surface; magnetic stirring was added under the reaction vessel to make the solution Mix well, keep the concentration and temperature uniform, catalyst TiO 2 /g-C 3 N 4 The dosage is 1g/L and the initial concentration of methylene blue is 20mg/L. After 1h, the concentration of methylene blue is 1.108mg/L, and the photocatalytic degradation rate of methylene blue reaches 94.46%.

Example

[0042] (Example 2)

[0043] Preparation of TiO in this example 2 /g-C 3 N 4 The rest of the method of composite visible light catalyst is the same as that of Example 1, except that: Ti(OBu) in step ① 4 The added amount is 5mL, the temperature of ethanol is 25°C, and the temperature of the water bath is 85°C.

[0044] Detected by X-ray diffractometer, the product of this example is g-C 3 N 4 , Anatase TiO 2 And rutile TiO 2 The mixture of crystals indicates that TiO was successfully prepared in this example 2 /g-C 3 N 4 Composite visible light catalyst.

[0045] TiO prepared in this example 2 /g-C 3 N 4 The TEM spectrum of the composite visible light catalyst shows nano-TiO 2 Particles are evenly distributed in graphite flake g-C 3 N 4 in.

[0046] Detected by ultraviolet-visible spectrometer, the TiO synthesized in this example 2 /g-C 3 N 4 The visible light absorption region of the composite visible light catalyst ranges from 390 to 530 nm.

[0047] Detect the TiO prepared in this example according to the method of example 1. 2 /g-C 3 N 4 The photocatalytic performance of methylene blue, the photocatalytic degradation rate of methylene blue reaches 96.32%.

Example

[0048] (Example 3)

[0049] Preparation of TiO in this example 2 /g-C 3 N 4 The rest of the method of composite visible light catalyst is the same as that of Example 1, except that: Ti(OBu) in step ① 4 The added amount of 100mL, the dripped amount of water is 1000mL, and the temperature of the water bath is 85°C.

[0050] Detected by X-ray diffractometer, the product of this example is g-C 3 N 4 , Anatase TiO 2 And rutile TiO 2 The mixture of crystals indicates that TiO was successfully prepared in this example 2 /g-C 3 N 4 Composite visible light catalyst.

[0051] TiO prepared in this example 2 /g-C 3 N 4 The TEM spectrum of the composite visible light catalyst shows nano-TiO 2 Particles are evenly distributed in graphite flake g-C 3 N 4 in.

[0052] Detected by ultraviolet-visible spectrometer, the TiO synthesized in this example 2 /g-C 3 N 4 The visible light absorption region of the composite visible light catalyst ranges from 390 to 530 nm.

[0053] Detect the TiO prepared in this example according to the method of example 1. 2 /g-C 3 N 4 The photocatalytic performance, the photocatalytic degradation rate of methylene blue reaches 91.45%.

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Method for preparing TiO2/g-C3N4 composite visible light catalyst

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